CN112082939A - Method for directly stretching and measuring film adhesion energy based on nano-indentation technology - Google Patents
Method for directly stretching and measuring film adhesion energy based on nano-indentation technology Download PDFInfo
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Abstract
The invention relates to a method for measuring the adhesion energy of a film by direct stretching based on a nanometer pressing-in technology, which comprises the steps of etching an I-shaped film cross section sample by utilizing the existing focused ion beam, welding the sample to a Push-to-Pull (PTP) device, then directly stretching in a single direction based on the nanometer pressing-in technology, and correcting stress displacement data to obtain the adhesion energy of the film. Compared with the prior art, the method has the advantages of direct quantitative measurement of the adhesion force of the film material and the substrate, simple data analysis process, high measurement precision and the like.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to a method for directly stretching and measuring the adhesion energy of a film based on a nanometer pressing-in technology.
Background
The film has unique properties (such as corrosion resistance, high temperature resistance, wear resistance, oxidation resistance, high hardness, attractive appearance and the like) and can be completely exposed in various fields, and relates to the fields of microelectronic semiconductor industry, aerospace, medical instruments, mechanical industry, nuclear energy and the like. Researchers in various fields often focus on the reliability of the film-substrate system, focusing on the film properties themselves, but not as much as the failure problem of film-substrate interfacial adhesion. Since the overall performance, structure, lifetime and durability of the product are highly dependent on the film-substrate adhesion properties, in order to obtain a strong interface, the adhesion of the film needs to be measured accurately.
The nano-indentation technology has the advantages of simple operation, nondestructive detection, high sensitivity, high precision and the like, provides a method for researching a thin film on a small scale, and is an important technology for measuring mechanical property parameters of materials. At present, nanoindentation has been widely applied to aspects such as characterization of hardness and elastic modulus, measurement of residual stress, characterization of film creep behavior, stress-strain, measurement of film thickness according to an unloading curve, and the like. With the development and further research of instruments, the application range of nano-indentation instruments is continuously expanded due to unique advantages, and in the aspect of interface adhesion, methods related to nano-indentation technology, such as an indentation method, a scratching method, a method for combining and covering a stress surface and the like, are common. Although the measurement of film adhesion has been hundreds of ways to date, there is no generally accepted method. Most tests depend on analysis models and assumptions, the size of cracks needs to be measured, the operation is complicated, the cracks are easily influenced by various factors, and many methods have poor repeatability or difficult data interpretation and cannot obtain visual quantitative data. In addition, in the use process of the traditional indentation method and the traditional scratch method, critical stress appears in the characterization result to be used for indirectly judging the adhesion performance, however, films (such as metal titanium, aluminum and the like) with excellent plasticity and adhesion cannot generate critical transformation in indentation and scratch tests, so that the adhesion cannot be measured.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for directly measuring the adhesion energy of a film by stretching based on a nano-indentation technology, which can directly and quantitatively measure the adhesion of a film material and a substrate and has the advantages of simple test steps, high repeatability, wider application range and the like.
The purpose of the invention can be realized by the following technical scheme:
a method for measuring the adhesion energy of a film by direct stretching based on a nano-indentation technology comprises the following steps:
s1: placing the film on a sample table inclined at 52 degrees, depositing a Pt protective layer on a position of interest on the surface of the film by utilizing a Focused Ion Beam (FIB) technology, hollowing out a rectangular groove along the upper edge and the lower edge of the Pt protective layer, roughly cutting out the cross section of the film-interface-substrate, and depositing the film on the substrate through magnetron sputtering; then, a finish cutting operation is performed for the cross-section switching surface cleaning mode.
The specific content of the fine cutting operation is as follows: the sample stage is rotated according to the angle range of +/-1.5 degrees on the basis of the original sample stage inclined by 52 degrees, the cleaning depth is 1um, and finally the sample with the thickness of about 1.5um is obtained through thinning.
S2: and (3) inclining the sample table to 7 degrees, after the film after rough cutting operation and fine cutting operation is subjected to U-shaped cutting, horizontally placing the sample table, inserting a sampling probe, taking out, and obtaining a sheet sample which is welded on the sampling probe and is parallel to the sampling probe.
S3: and etching the I-shaped tensile sample on the thin sheet sample by utilizing a focused ion beam technology.
S4: the i-shaped tensile sample, now parallel to the sampling probe, is welded to a vertically placed metal medium and cut apart from the sampling probe.
S5: and adjusting the metal medium to be horizontally placed, re-inserting the needle to enable the sampling probe to form 45 degrees with the surface of the I-shaped tensile sample, and re-extracting the sample.
S6: the I-shaped tensile sample is placed on a Push-to-Pull (PTP) device, an upper wing plate and a lower wing plate of the I-shaped tensile sample are respectively arranged corresponding to the PTP device plate, a web plate is suspended, the film-substrate interface of the web plate is positioned in the middle of a gap, Pt welding spots are stacked around the upper wing plate and the lower wing plate of the sample by utilizing a focused ion beam technology, and the Pt welding spots are welded to the PTP device.
S7: and pressing down the semicircular end part at the top of the PTP device by using a pressure head of a nanometer pressing-in technology, and recording load-displacement while stretching the sample in a single direction until the critical load is reached, wherein the interface fracture occurs.
S8: and correcting the real displacement and the real stress, and calculating the interface adhesion energy.
Formula G calculated for interfacial adhesion energy is:
σt＝σe(1+e)
wherein Δ l is the true displacement, FtIn order to apply the actual force on the sample,
f is the recorded load, x is the total displacement, K1Rigidity of PTP plant at no load, K2The rigidity of the PTP device when the PTP device is not unloaded; sigmatIs true stress, σeIn order to achieve the engineering stress,
ein order to achieve the engineering strain,
Eeffis effective elastic modulus of the film-substrate, satisfies
EfIs the modulus of elasticity of the film, EsIs the elastic modulus of the substrate, /)0Is the original height of the web, A0Is the initial cross-sectional area.
Further, the length of the Pt protective layer for deposition is 8um, the width is 2um, and the height is 1 um.
Further, the upper and lower rectangular grooves are hollowed from the outside to the edge of the Pt protective layer, wherein the length of each rectangular groove is 12um, the depth of each rectangular groove is 2um deeper than the depth of the measured film-substrate interface, and the width of each rectangular groove is 2 times the depth of each rectangular groove.
Further, the total length size range of the I-shaped stretching sample is 7-8 um, the width is 1.5um, the total height is the sum of the thickness of a Pt protective layer, the thickness of a film and the thickness of a substrate, the height of upper and lower wing plates is required to be the same, the length size range of a web plate is 0.8-1.5 um, the original height of the web plate is the same as the gap size of a PTP device, and the film-substrate interface is ensured to be on the web plate.
Further, the metal medium includes a copper mesh.
Further, the indenter of the nanoimprint technology is a flat indenter, and operates at a displacement rate of 2nm/s in a displacement control mode.
Compared with the prior art, the method for directly measuring the film adhesion energy based on the nanometer pressing-in technology at least comprises the following beneficial effects:
firstly, micromachining an I-shaped tensile sample containing an interface by using an FIB technology, skillfully utilizing the advantages of a PTP device in the technology of converting and pushing into pulling and nano pressing to accurately measure load and displacement, and returning the measurement method of the adhesion energy of the complex film to the most original direct tensile test; by matching with the calculation formula provided by the invention, the adhesion energy of the film material and the substrate can be measured most directly and quantitatively; the test process does not need to preset cracks and measure the sizes of the cracks, and the test step is simple and has high repeatability.
Compared with the existing methods (such as an indentation method and a scratching method) which need to use hypothesis and a complex mechanical model, the method provided by the invention provides a new film adhesion energy formula according to the elastic energy, the obtained result has high precision, and direct, effective and accurate parameter evaluation can be provided for the measurement of the adhesion energy of the material.
And thirdly, the direct stretching method is suitable for various film material types, and compared with the traditional indentation method and the traditional scratch method, the direct stretching method is effective for the adhesion performance test of any film material and has wider application range, and the adhesion performance can be indirectly judged only by representing the critical stress in the result.
Drawings
FIG. 1 is a schematic diagram of the working principle of the method for measuring the adhesion energy of a film by direct stretching based on the nano-indentation technology according to the present invention;
FIG. 2 is a stress-displacement curve of a tungsten film-single crystal silicon substrate in an example;
FIG. 3 is a stress-displacement curve of a W-Ti film-single crystal silicon substrate according to an embodiment;
FIG. 4 is an SEM image of the interface fracture of the tungsten film-single crystal silicon substrate in the example.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of protection of the present invention.
Examples
As shown in FIG. 1, the invention relates to a method for directly stretching and measuring the adhesion energy of a film based on a nano-indentation technology, which comprises the following steps:
The precision cutting is that the sample table is adjusted to +/-1.5 degrees in sequence on the basis of the original sample table inclined at 52 degrees, the cleaning depth is 1um, and finally the sample with the thickness of about 1.5um is obtained by thinning.
And 2, inclining the sample table to 7 degrees, cutting the film sample processed in the step 1 into a U shape, horizontally placing the sample table, and taking out the film sample through the sampling probe to obtain a sheet sample which is adhered to the sampling probe and is parallel to the sampling probe.
And 3, etching the slice sample obtained in the step 2 by using an FIB (focused ion beam) technology to obtain an I-shaped stretched sample.
And 4, welding the I-shaped tensile sample parallel to the sampling probe to a vertically placed metal medium, and cutting and separating the sample and the sampling probe.
And 5, adjusting the metal medium to be horizontally placed for conveniently placing the sample subsequently, inserting the needle again, enabling the sampling probe to form an angle of 45 degrees with the surface of the I-shaped stretched sample, and then re-extracting the sample.
And 6, placing the I-shaped tensile sample on a Push-to-Pull (PTP) device, arranging the upper wing plate and the lower wing plate of the I-shaped tensile sample respectively corresponding to the plates of the PTP device, suspending the web plate, placing the film-substrate interface in the middle of the gap, stacking Pt welding spots around the upper wing plate and the lower wing plate of the sample by using a focused ion beam technology, and welding the Pt welding spots to the PTP device.
And 7, pressing down the semicircular end part at the top of the PTP device by using a pressure head of a nanometer pressing-in technology, and recording the load-displacement while stretching the sample in a single direction until the critical load is reached, wherein the interface is broken.
Step 8, calculating the interface adhesion energy G according to the following formula:
σt＝σe(1+e) (2)
where Δ l is the true displacement, the true force exerted on the sample
F is the recording load, x is the total displacement, K1Is the rigidity of the PTP plant at no load, K2Is the stiffness, σ, of the PTP devicetIs true stress, engineering stress
Engineering strain
Effective modulus of elasticity of film-substrate
EfIs the modulus of elasticity of the film, EsIs the modulus of elasticity of the substrate, /)0Is the original height of the web, A0Is the initial cross-sectional area.
In step 1, a thin film is deposited on a substrate by magnetron sputtering.
As a preferred scheme, the deposited Pt protective layer has the length of 8um, the width of 2um and the height of 1 um. The hollowing directions of the upper rectangular groove and the lower rectangular groove are from the outer side to the edge of the Pt protective layer, the length of each rectangular groove is 12 microns, the depth of each rectangular groove is 2 microns deeper than the depth of a measured film-substrate interface, and the width of each rectangular groove is 2 times of the depth; the essence is cut and is rotated sample platform 1.5 in proper order on the basis of original 52 sample platforms that incline, and clean degree of depth is 1um, and the sample of thickness about 1.5um is obtained to final attenuate. The total length size range of the 'I-shaped' stretching sample is 7-8 microns, the width is 1.5 microns, the total height is the sum of the thickness of a Pt protective layer, the thickness of a film and the thickness of a substrate, the height of upper and lower wing plates is required to be the same, the length size range of a web plate is 0.8-1.5 microns, the original height of the web plate is the same as the gap size of a PTP device, and the film-substrate interface is ensured to be on the web plate. The metal media comprises a copper mesh. The pressure head of the nanometer pressing technology is a flat pressure head and operates at a displacement rate of 2nm/s in a displacement control mode.
The length of the Pt protective layer is selected as empirical data for easy observation and ion thinning. If the ion thickness is too small, the observation area is small, and if the ion thickness is too large, the ion thickness reduction needs longer time, and errors are easy to occur. The length of the rectangular groove is 12um, because the length of the Pt protective layer is 8um, two sides of the Pt protective layer are left to be 2um or so, and U-shaped cutting is convenient; the width is selected so that when the subsequent sample stage is adjusted from 52 degrees to 7 degrees, the bottom can be conveniently observed, the U-shaped cutting range of the bottom of the slice can be accurately planned, and the focused ion beam can not touch the peripheral film. The 52 degree setting is to match the inclination angle of the focused ion beam when the focused ion beam is installed, and the focused ion beam is vertically hollowed, so that the section is not smooth, and the bottom is remained and not smooth (as can be seen from the side view of the subgraph (1) in fig. 1); the auxiliary tilt is set to ± 1.5 °, and the cleaning depth is set to 1um to thin the bottom of the wafer.
The overall height of the I-shaped tensile sample is theoretically unlimited, the total height is the sum of the thickness of the Pt protective layer, the thickness of the film and the thickness of the substrate, the height of the upper wing plate and the height of the lower wing plate are required to be the same, and the thickness range of the tested film is expanded. In principle it is only necessary that the film-substrate interface be on the web (i.e. in the PTP device gap). The length and width of the web are both 1.5um, and small-area fracture is easier to occur at the interface, so that the possibility of other types of fracture is reduced.
The present invention is further illustrated by the following examples, which are intended to be illustrative only and not to limit the scope of the invention.
Firstly, in this embodiment, according to the method for directly measuring the adhesion energy of the thin film by stretching based on the nanoimprint technology, the adhesion energy of the tungsten film-monocrystalline silicon substrate is directly measured by stretching, and the specific measurement process is as follows:
before sputtering, a monocrystalline silicon substrate is placed in absolute ethyl alcohol, ultrasonic cleaning is carried out for 5 minutes, a tungsten film is deposited on the monocrystalline silicon substrate through direct-current magnetron sputtering, and the target material is 99.9% of pure tungsten. Vacuum pumping to 1.0^10 during sputtering-5And (3) torr, introducing pure Ar gas, sputtering power of 200w, and alternately sputtering at high pressure and low pressure (15mtorr, 10min and 2mtorr, 10min) to obtain a 2.5um tungsten film.
Roughly cutting (the size of an upper rectangular groove is 12um multiplied by 7um multiplied by 4um, the size of a lower rectangular groove is 12um multiplied by 8um multiplied by 4.5um) by using a focused ion beam in sequence, finely cutting and etching to obtain an I-shaped sample (the integral size of the I-shaped sample is 7um multiplied by 1.5um multiplied by 6um, the heights of an upper wing plate and a lower wing plate are the same, the size of a web plate is 0.8um multiplied by 2.5um multiplied by 1.5um), overturning a copper mesh, and welding to a PTP device to prepare a micron-sized tensile sample; placing the sample in a nanoindentation instrument, adopting a flat pressure head, operating the pressure head at a displacement rate of 2nm/s in a displacement control mode, pressing down the semicircular end part at the top of the PTP device, ensuring that the thermal expansion is about 0.4nm/s, and ensuring that the rigidity K is realized when the PTP device is in no-load10.3846uN/nm, stiffness K of PTP device2104.6uN/nm, the true displacement Δ l and the true stress σ are corrected according to the equations (1) and (2)tAnd drawing a stress-displacement curve as shown in fig. 2, and drawing an interface fracture diagram of the tungsten film-monocrystalline silicon substrate as shown in fig. 4, and confirming that the measured data is actually the interface value of the tungsten film and the monocrystalline silicon substrate.
Obtaining adhesion energy G according to the formula (3)1＝18.54J/m2。
Then, in this embodiment, according to the method for directly measuring the adhesion energy of the thin film by stretching based on the nanoimprint technology, the adhesion energy of the tungsten-titanium-single crystal silicon substrate is directly measured by stretching, and the specific measurement process is as follows:
before sputtering, a monocrystalline silicon substrate is placed in absolute ethyl alcohol, ultrasonic cleaning is carried out for 5 minutes, pure titanium is deposited on the monocrystalline silicon substrate through radio frequency magnetron sputtering, and the target material is 99.9 percent of pure titanium. During sputtering, the vacuum pumping is carried out until the pressure reaches 1.0^10-5torr, pure Ar gas is introduced, the sputtering power is 150w, and the sputtering time is 150s, so as to obtain a layer of pure titanium-monocrystalline silicon substrate. And depositing a tungsten film on the monocrystalline silicon substrate by direct-current magnetron sputtering, wherein the target material is 99.9% of pure tungsten. The sputtering power is 200w, high-low voltage alternate sputtering (15mtorr, 10min and 2mtorr, 10min) is carried out, and the tungsten-titanium film with the total thickness of 2.6um is obtained.
Roughly cutting (the size of an upper rectangular groove is 12um multiplied by 7um multiplied by 4um, the size of a lower rectangular groove is 12um multiplied by 8um multiplied by 4.5um) by using a focused ion beam in sequence, finely cutting and etching to obtain an I-shaped sample (the integral size of the I-shaped sample is 7um multiplied by 1.5um multiplied by 6.5um, the heights of an upper wing plate and a lower wing plate are the same, the size of a web plate is 1.1um multiplied by 2.5um multiplied by 1.5um), overturning a copper mesh, and welding to a PTP device to prepare a micron-sized tensile sample; placing a sample in a nano indentation instrument, adopting a flat pressure head, operating the pressure head at a displacement rate of 2nm/s in a displacement control mode, pressing down a semicircular end part at the top of a PTP device, ensuring that the thermal expansion is about 0.4nm/s, the rigidity K1 is 0.3846uN/nm when the PTP device is unloaded, the rigidity K2 is 104.6uN/nm, and correcting the real displacement delta l and the real stress sigma according to the formulas (1) and (2)tThe stress-displacement curve is plotted as shown in fig. 3.
Obtaining adhesion energy G according to the formula (3)2＝22.59J/m2From G1＜G2It is known that the titanium transition layer increases the interfacial adhesion between the tungsten film and the silicon substrate.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and those skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for directly measuring the adhesion energy of a film by stretching based on a nano-indentation technology is characterized by comprising the following steps:
1) placing the film on a sample table inclined at 52 degrees, depositing a Pt protective layer on a position of interest on the surface of the film by utilizing a focused ion beam technology, hollowing out a rectangular groove along the upper edge and the lower edge of the Pt protective layer, roughly cutting out the cross section of the film-interface-substrate, and then carrying out fine cutting operation on the cross section by switching a surface cleaning mode;
2) inclining the sample table to 7 degrees, after performing U-shaped cutting on the film subjected to rough cutting operation and fine cutting operation, horizontally placing the sample table, inserting a sampling probe, taking out, and obtaining a sheet sample which is welded on the sampling probe and is parallel to the sampling probe;
3) etching the sheet sample by utilizing a focused ion beam technology to obtain an I-shaped tensile sample;
4) welding an I-shaped tensile sample parallel to the sampling probe to a vertically placed metal medium, and cutting and separating the I-shaped tensile sample and the sampling probe;
5) adjusting the metal medium to be horizontally placed, re-inserting the needle to enable the sampling probe to form 45 degrees with the surface of the I-shaped tensile sample, and re-extracting the sample;
6) placing an I-shaped tensile sample on a PTP device, arranging an upper wing plate and a lower wing plate of the I-shaped tensile sample respectively corresponding to the PTP device plates, suspending a web plate, positioning a film-substrate interface of the web plate in the middle of a gap, stacking Pt welding spots around the upper wing plate and the lower wing plate of the sample by utilizing a focused ion beam technology, and welding the Pt welding spots to the PTP device;
7) pressing down the semicircular end part at the top of the PTP device by using a pressure head of a nanometer pressing-in technology, and recording load-displacement while stretching the sample in a single direction until the critical load is reached, wherein the interface fracture occurs;
8) and correcting the real displacement and the real stress, and calculating the interface adhesion energy.
2. The method for direct tensile measurement of film adhesion energy based on nanoimprint technology of claim 1, wherein the calculation formula G of interfacial adhesion energy is:
σt＝σe(1+e)
G＝∫0 ΔlσtdΔl
wherein Δ l is the true displacement, FtIn order to apply the actual force on the sample,
f is the recorded load, x is the total displacement, K1Rigidity of PTP plant at no load, K2The rigidity of the PTP device when the PTP device is not unloaded; sigmatIs true stress, σeIn order to achieve the engineering stress,
ein order to achieve the engineering strain,
Eeffis effective elastic modulus of the film-substrate, satisfies
EfIs the modulus of elasticity of the film, EsIs the elastic modulus of the substrate, /)0Is the original height of the web, A0Is the initial cross-sectional area.
3. The method for direct tensile measurement of film adhesion energy based on nanoimprint technology of claim 1 wherein, in step 1), the film is deposited on the substrate by magnetron sputtering.
4. The method for direct tensile measurement of film adhesion energy based on nanoimprint technology of claim 1, wherein in step 1), the Pt protective layer used for deposition has a length of 8um, a width of 2um, and a height of 1 um.
5. The method for direct tensile measurement of film adhesion energy based on nanoimprint technology of claim 1, wherein in step 1), the upper and lower rectangular grooves are hollowed in the direction from the outside to the edge of the Pt protective layer, wherein the length of each rectangular groove is 12 μm, the depth of each rectangular groove is 2 μm deeper than the depth of the film-substrate interface to be measured, and the width of each rectangular groove is 2 times the depth of each rectangular groove.
6. The method for directly measuring the adhesion energy of the film based on the nano-indentation technology as claimed in claim 1, wherein in the step 1), the precise cutting operation comprises: the sample stage is rotated according to the angle range of +/-1.5 degrees on the basis of the original sample stage inclined by 52 degrees, the cleaning depth is 1um, and finally the sample with the thickness of about 1.5um is obtained through thinning.
7. The method for directly stretching and measuring the adhesion energy of the thin film based on the nanoimprint technology as claimed in claim 1, wherein the length dimension of the I-shaped stretched sample is in the range of 7-8 um, the width of the I-shaped stretched sample is 1.5um, and the total height is the sum of the thickness of the Pt protective layer, the thickness of the thin film and the thickness of the substrate.
8. The method for directly measuring the film adhesion energy based on the nano-indentation technology as claimed in claim 7, wherein the heights of the upper and lower wing plates of the I-shaped tensile sample are the same, the length dimension of the web is in the range of 0.8-1.5 um, and the original height of the web is the same as the gap dimension of the PTP device.
9. The method for direct tensile measurement of film adhesion energy based on nanoimprint technology of claim 1 wherein the metallic media comprises copper mesh.
10. The method for directly measuring the adhesion energy of the thin film based on the nano-indentation technology as claimed in claim 1, wherein the indenter of the nano-indentation technology in step 7) is a flat indenter, and is operated at a displacement rate of 2nm/s in a displacement control mode.
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| CN114965004A (en) * | 2021-02-25 | 2022-08-30 | 胜科纳米（苏州）有限公司 | Patterning test method for interface bonding force of device-level nano film layer |
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| CN112798822A (en) * | 2021-01-13 | 2021-05-14 | 国家纳米科学中心 | Method for testing bending stiffness of two-dimensional nano material and interface adhesion performance between two-dimensional nano material and substrate |
| CN112798822B (en) * | 2021-01-13 | 2022-06-17 | 国家纳米科学中心 | Method for testing bending stiffness of two-dimensional nano material and adhesion performance of interface between two-dimensional nano material and substrate |
| CN114965004A (en) * | 2021-02-25 | 2022-08-30 | 胜科纳米（苏州）有限公司 | Patterning test method for interface bonding force of device-level nano film layer |
| CN113075047A (en) * | 2021-03-30 | 2021-07-06 | 重庆大学 | Method for determining elastic energy of circular film under gas pressure |
| CN113075047B (en) * | 2021-03-30 | 2022-03-25 | 重庆大学 | Method for determining elastic energy of circular film under gas pressure |
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